EP0483579B1 - Sonde d'échelle nanomètre pour microscope à force atomique, et méthode de fabrication - Google Patents

Sonde d'échelle nanomètre pour microscope à force atomique, et méthode de fabrication Download PDF

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Publication number
EP0483579B1
EP0483579B1 EP91117499A EP91117499A EP0483579B1 EP 0483579 B1 EP0483579 B1 EP 0483579B1 EP 91117499 A EP91117499 A EP 91117499A EP 91117499 A EP91117499 A EP 91117499A EP 0483579 B1 EP0483579 B1 EP 0483579B1
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European Patent Office
Prior art keywords
probe
substrate
tip
needle
recited
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Expired - Lifetime
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EP91117499A
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German (de)
English (en)
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EP0483579A3 (fr
EP0483579A2 (fr
Inventor
Joachim G. Clabes
Michael Hatzakis
Kam L. Lee
Bojan Petek
John C. Slonczewski
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International Business Machines Corp
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International Business Machines Corp
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
    • G01Q70/00—General aspects of SPM probes, their manufacture or their related instrumentation, insofar as they are not specially adapted to a single SPM technique covered by group G01Q60/00
    • G01Q70/08—Probe characteristics
    • G01Q70/10—Shape or taper
    • G01Q70/12—Nanotube tips
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
    • G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
    • G01Q60/50—MFM [Magnetic Force Microscopy] or apparatus therefor, e.g. MFM probes
    • G01Q60/54—Probes, their manufacture, or their related instrumentation, e.g. holders
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R1/00—Details of instruments or arrangements of the types included in groups G01R5/00 - G01R13/00 and G01R31/00
    • G01R1/02—General constructional details
    • G01R1/06—Measuring leads; Measuring probes
    • G01R1/067—Measuring probes
    • G01R1/07—Non contact-making probes

Definitions

  • This invention relates to atomic force microscopy, and more particularly, to a nanometer scale probe for use with an atomic force microscope.
  • Scanned probe microscopy saw its commencement at the atomic level with the invention by Binnig et al. of the scanning tunnelling microscope in the mid-1980's.
  • STM scanning tunnelling microscope
  • a tiny tungsten probe is maneuvered to within a nanometer above the surface of a conducting specimen, sufficiently close so that there is an overlap between the electron clouds of the atom at the probe tip and of the nearest atom of the specimen.
  • When a small voltage is applied to the tip electrons "tunnel” across the gap generating a small tunnelling current. The strength of that current is very sensitive to the width of the gap.
  • Piezoelectric controls are used to control the motion of the probe and move it back and forth across the specimen while maintaining a constant gap between its tip and the specimen surface. The variations in voltage applied to maintain the probe properly positioned over the surface are electronically translated into an image of the surface topography.
  • the invention of STM has led to the development of a family of new scanned-probe microscopes, one of which is the atomic force microscope (AFM) which negates the need for a conducting specimen.
  • the AFM relied upon the repulsive forces generated by the overlap of the electron cloud at the tip's surface with electron clouds of surface atoms within the specimen.
  • the tip is mounted on a flexible beam which maintains the tip pressed against the specimen surface with constant force as it is moved across the surface.
  • AFM that is based on the detection of an attractive force between a surface and a probe by its effect on the dynamics of a vibrating probe/beam arrangement.
  • a tapered tungsten wire is driven by a piezoelectric transducer mounted at its base to vibrate at close to the wire's resonant frequency.
  • amplitude changes occur in the vibration as a result of the attractive forces.
  • the changes in the vibration amplitude are sensed by an interferometric laser arrangement.
  • FIG. 1 A block diagram of an AFM using interferometric laser detection is shown in Fig. 1, with a probe arrangement 10 being emplaced over the surface of specimen 12. Changes in oscillation amplitude of probe arrangement 10 are sensed by a laser heterodyne interferometer 14 that provides an output signal to a feedback generator 16. As an output signal changes with respect to an applied reference signal, feedback generator 16 provides position control signals to a piezoelectric position control unit 18. Those control signals cause a piezoelectric unit within position control element 18 to move the specimen so that the vibration amplitude is stabilized and, hence the the force gradient. The fluctuations in the feedback potential are converted into a profile of the surface being investigated.
  • AFM electrostatic-force microscope
  • the vibrating probe bears an electric charge and its vibration amplitude is effected by electrostatic forces resulting from charges in the sample.
  • AFM Magnetic-force microscope
  • MFM magnetic-force microscope
  • a magnetized nickel or iron probe is substituted for the tungsten or silicon needles used with other AFM's.
  • the tip feels a magnetic force that changes its resonance frequency and hence its vibration amplitude.
  • the MFM traces magnetic-field patterns emanating from the specimen.
  • the magnetic force components sensed by an MFM probe result from the interaction of the total magnetic dipole moments at the tip of the probe and the specimen. They are further dependent upon the influence of tip-related magnetic fields on the local magnetic moments of the specimen.
  • the lateral resolution of the probe depends critically on the interaction volume constituted by the sample and the tip. For planar magnetic media, this interaction volume is determined primarily by geometric and magnetic properties of the probe tip. Thus, in order to obtain lateral resolutions below 100,0 nm, current tip sizes in the range of 100,0 nm are too large.
  • magnetic sensor probe tips are fabricated by an electrochemical etching technique using a ferromagnetic wire material (such as nickel, iron, or cobalt). Essentially the method comprises etching the tip of the wire until it approximates a point. This method does not provide control over the geometric shape of the tip below a 100,0 nm radius. Such probe tips, further, have an unnecessarily large amount of magnetic material with a complicated domain structure. In essence, subtractive processes for creating MFM and other AFM probe tips, do not today, provide the desired atomic-level resolution capability.
  • a ferromagnetic wire material such as nickel, iron, or cobalt
  • a film is deposited on a semiconductor substrate by passing a gas containing an element over the substrate and then irradiating a determined portion thereof with an electron beam. The gas decomposes and the element is precipitated onto the substrate so as to form a desired pattern. Chromium, molybdenum, aluminum, and tungsten containing organometallics are disclosed. In Japanese Patent 87-295,886/42 the use of organometallic compounds is described for producing a film of VIII metals on a substrate. Electron beams have also been used to enable surface analysis of substrates (e.g., see Kuptsis, IBM Technical Disclosure Bulletin, Vol. 13, No. 9, February 1971, pp. 2497-2498).
  • a probe tip for a scanned probe microscope is configured as a needle extending from a surface, the needle further comprising a carbonized matrix of a decomposed organic reactant.
  • the needle exhibits a substantial stiffness along its elongated dimension and has a nanometer scale tip dimension.
  • a method is described for producing such a needle probe tip wherein a substrate is positioned in an evacuated environment; a volatile organic compound is introduced into the environment and an energy beam, for example a laser beam, an electron beam or an x-ray beam from a synchrotron and the like, is directed at the substrate's surface, which energy beam is maintained stably focussed thereon for a preset time period.
  • the beam causes a selective decomposition of the organic compound at the focal point on the substrate surface and causes succeeding layers of decomposition product of the organic compound to grow directly up the beam, to thus produce a substantially rigid nanometer-scale needle-like form.
  • a magnetic layer is then deposited on the top of the structure, such layer having a dimension which restricts the tip to exhibit a single magnetic domain.
  • FIG. 2 the structure of an AFM nanometer scale needle probe will be described, including the process for producing such a probe.
  • a substrate 20 is placed in an evacuated chamber within an electron beam unit.
  • substrate 20 is a silicon cone.
  • a volatile, organometallic compound gas stream is then introduced into the subchamber 64, while at the same time, an electron beam 22 is turned on. Beam 22 impinges upon an upper surface 24 of substrate 20 and causes decomposition and preferential deposition of the decomposed products of the organometallic gas onto surface 24. Such deposition occurs within the region irradiated by electron beam 22 and also out therefrom by a radial distance determined by electron scatter from surface 24. If it is assumed that electron beam 22 has a diameter of 6 nanometers, the diameter of the initial deposit is approximately 100 nanometers. As the process continues, additional layers of deposited, decomposed components of the organometallic gas continue to build up, thereby creating a needle-like shape 26.
  • a conical tip shape for needle 26 and its shank diameter are achieved by control of the primary beam voltage and also the beam's gaussian profile.
  • the needle diameter and the respective cone apex angle decrease with increasing beam voltage ( ⁇ 10% for a 10 kV increase).
  • Such a needle shape is shown in Fig. 3(a).
  • the apparent diameter of pointed end 28 of needle 26 can be made approximately 10 nanometers.
  • the process employed to deposit needle probe 26 onto a substrate is an electron beam chemical vapor deposition (CVD) process.
  • CVD electron beam chemical vapor deposition
  • Such processes, per se, are known in the prior art, e.g., see Japanese Patent 87-295,886/42. Nevertheless, to Applicants' knowledge, such processes have not heretofore been employed to produce nanometer scale, needle-like structures having a high aspect ratio.
  • the E-beam CVD process produces a needle probe which exhibits substantial stiffness along its elongated dimension. It is believed that this rigidity results from the CVD process producing a needle with a carbon matrix structure in which metal particles are dispersed. In other words, the included carbon toughens the structure and makes it usable as an AFM probe. Without such structural stiffness, needle probe 26 would be useless as an AFM probe.
  • metal carbonyls or metal alkyls can be employed as organometallic source compounds for the CVD process, it is preferred that metallocenes be employed due to the non-thermal, decomposition process occuring under e-beam irradiation.
  • metallocenes be employed due to the non-thermal, decomposition process occuring under e-beam irradiation.
  • cobaltocene, nickelocene, and/or ferrocene are preferred.
  • a needle structure such as shown in Fig. 3(a) is grown and exhibits intrinsic, but weak, magnetic capabilities.
  • Such needle structure comprises a carbon matrix with nickel, cobalt or iron particles, as the case may be, dispersed therein.
  • a seeding step followed by a plate-up of a magnetic material.
  • a seeding material e.g., allycyclopentadienylpalladium
  • a seeding material is used to grow needle 26 (see Fig. 3(b)). This results in a non-magnetic needle structure having palladium seed particles interspersed.
  • the entire surface of needle 26 is then covered, in a subsequent electroless plating process, by a magnetic metal layer 30.
  • the needle 26 is grown without an included metal component. Then a seeding material 32 is deposited only on the apex of needle 26. This is accomplished by introduction of a gaseous metallorganic containing the seed metal, followed by electron beam exposure of the tip area. A subsequent plating (e.g. selective CVD in a gaseous or liquid environment) of a magnetic metal 30 will therefore be confined to the seeded area at the apex and will yield a single domain magnetic sensor region for needle probe 26.
  • a seeding material 32 is deposited only on the apex of needle 26. This is accomplished by introduction of a gaseous metallorganic containing the seed metal, followed by electron beam exposure of the tip area.
  • a subsequent plating (e.g. selective CVD in a gaseous or liquid environment) of a magnetic metal 30 will therefore be confined to the seeded area at the apex and will yield a single domain magnetic sensor region for needle probe 26.
  • Fig. 4 a perspective view taken from an SEM photograph is shown wherein a 3 micron long needle probe with a 100 nanometer shank diameter was produced using the method of this invention.
  • the substrate is a silicon pedestal produced via selective etching.
  • Silicon probe tips such as tip 20 shown in Fig. 2 or the one shown in Fig. 4, are produced by microfabrication techniques that are known in the art. For instance, see Albrecht et al., "Microfabrication of Cantilever Styli for the Atomic Force Microscope", Journal of Vacuum Science Technology, A8(4), July/August 1990, pp. 3386-3396. In that reference and in the references cited therein, techniques are described for selective etching of silicon substrates to enable the creation of an AFM cantilever with an integral pointed silicon probe tip. The procedures used to provide such integral cantilever/probe structures employ selective etching and mask undercutting to enable production of the probe tips. The Albrecht et al. article also describes methods for fabricating thin film SiO2 and Si3N4 microcantilevers having integral probe tips. Such procedures do not form a part of this invention, although they do provide the methods and procedures whereby an appropriate support surface for the needle probe of this invention can be produced.
  • a direct E-beam deposition system comprises a modified scanning electron microscope.
  • the column portion of the microscope includes a filament 40 which is preferably a lanthanum boride electron source.
  • a movable anode structure 42 is provided to enable the beam brightness to be optimized.
  • the beam passes through a pair of condenser lenses 44, 46, double deflection coils 48 and a final lens 50. From there, the beam enters a lower chamber 52, passes through a backscatter electron detector 54 and then passes into and through a retractable shutter arrangement 56.
  • a linear drive mechanism 59 controls the position of the retractable shutter.
  • the shutter is closed and the beam passes through a pin hole therein (not shown).
  • a pin hole therein not shown.
  • Substrate 58 is positioned in subchamber 64 and on a Peltier effect heater/cooler 60 which maintains constant its temperature.
  • a vapor source 62 provides a vapor of an organometallic containing gas into subchamber 64.
  • a capacitance manometer 66 maintains the pressure within subchamber 64 within desired limits.
  • Various detection systems are included, including a secondary electron detector 66 and a STEM detector 68.
  • the position of substrate 58 is controlled by an XYZ stage 70 and controls that enable the discrete positioning of stage 70 (not shown).
  • the deposition system is interfaced to a pattern generating unit 72 which is controlled by a personal computer 74 to vector position the electron beam onto the substrate.
  • Electron beam on-time is controlled by an electrostatic blanking unit 76.
  • the exposure time per pixel ranges from 1 microsecond to greater than 100 seconds. For a 50X50 micron field, a beam step size of approximately 5 nanometers can be obtained with 14 bit digital to analog conversion.
  • Such control is exerted by field size control unit 78 through scan control amplifiers 80.
  • a source gas is introduced from vapor source 62 through a metering needle valve 63 into subchamber 64 within lower chamber 52.
  • Subchamber 64 is differentially pumped to an operating pressure range of 10-100 m Torr.
  • Such pressures are compatible with the available beam current densities, and enable optimum growth in the E-beams CVD process.
  • Typical pressure in SEM chamber 52 is approximately 133,3 ⁇ 10 ⁇ 4 N m2 (10 ⁇ 4 Torr) and the pressure in the gun area which encompasses source 40 is approximately 133,3 ⁇ 10 ⁇ 7 N m2 (10 ⁇ 7 Torr).
  • a weak magnetic probe needle comprised of nickel embedded in a carbon matrix, having a shank diameter of approximately 100 nanometers and length of two microns was deposited on a silicon substrate.
  • the organometallic gas used for this example was a nickelocene complex at a vapor pressure of 5 mTorr in subchamber 64.
  • the substrate temperature was 20°C
  • the beam voltage was 30 kV
  • the beam size diameter was approximately 6 nanometers.
  • the exposure time was between 5 and 10 minutes.
  • a strong magnetic needle sensor was produced under the following experimental conditions: A needle was first grown under same beam conditions and temperature as described above, using allycyclopentadienylpalladium complex as the vapor source material. Subsequently, the needle surface was plated in an electroless NiSO4 solution at 65°C yielding ⁇ 10nm nickel coverage in 5 seconds.
  • the above-described E-beam deposition process when applied to the deposition of a three-dimensional needle-like structure, has the unique characteristic of enabling monolayer film thickness control, high resolution, and the production of a high aspect ratio structure (i.e., more than 31). For most applications, it will probably be advantageous to produce an elongated magnetic tip shape, which would guarantee that the tip be magnetized along its long axis. Given the nanometer scale tip dimension, a single domain probe tip is achieved, enabling imaging of magnetic structures in the sample surface with atomic level resolution.

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  • General Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Radiology & Medical Imaging (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
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  • Measurement Of Length, Angles, Or The Like Using Electric Or Magnetic Means (AREA)
  • Length Measuring Devices With Unspecified Measuring Means (AREA)
  • Measuring Magnetic Variables (AREA)

Claims (13)

  1. Sonde pour un microscope à sonde à balayage, comprenant :
    un substrat (20, 58),
    une structure en forme d'aiguille (26) à échelle nanométrique ayant une pointe (28), présentant un allongement élevé, s'étendant depuis ledit substrat, ladite structure comprenant un matériau carbonisé, ladite structure présentant en outre une rigidité importante, caractérisée en ce que ledit matériau carbonisé comprend une matrice carbonisée de réactif organique décomposé et en ce que ladite structure en forme d'aiguille comporte un domaine magnétique unique sur ladite pointe.
  2. Sonde telle que décrite dans la revendication 1 dans laquelle ladite matrice carbonisée comprend des dépôts métalliques dispersés dans celle-ci.
  3. Sonde telle que décrite dans la revendication 2 dans laquelle lesdits dépôts métalliques présentent des propriétés magnétiques.
  4. Sonde telle que décrite dans la revendication 3 dans laquelle ladite structure présente un diamètre de sommet suffisamment petit pour qu'il puisse manifester sur celui-ci le domaine magnétique unique.
  5. Sonde telle que décrite dans la revendication 1 dans laquelle ledit substrat comprend un levier de soutènement flexible comportant une saillie intégrée s'étendant dans une direction perpendiculaire à celui-ci ladite saillie présentant une surface de sommet (24) à partir de laquelle s'étend ladite structure en forme d'aiguille (26).
  6. Sonde telle que décrite dans la revendication 5 dans laquelle ledit levier de soutènement flexible et la saillie sont composés de matériau à base de silicium.
  7. Sonde telle que décrite dans la revendication 1 comprenant en outre :
    une couche métallique fine disposée sur au moins une extrémité distale de ladite structure, ladite couche métallique fine présentant des propriétés magnétiques.
  8. Sonde telle que décrite dans la revendication 7 comprenant en outre :
    une fine intercouche contenant du métal disposée entre ladite extrémité distale de ladite structure et ladite couche magnétique métallique fine.
  9. Sonde telle que décrite dans l'une quelconque des revendications précédentes 1 à 8, dans laquelle ladite structure en forme d'aiguille a un allongement supérieur à environ 10 pour 1.
  10. Procédé pour créer une sonde pour un microscope à sonde à balayage, ladite sonde comprenant un substrat (20, 58) et une pointe de sonde supportée (28), le procédé comprenant :
    le positionnement dudit substrat (20, 58) dans un environnement de vide,
    l'introduction d'un composé à base organique, gazeux, volatil dans ledit environnement, dans lequel ledit composé à base organique contient un métal de germe,
    l'action de diriger un faisceau d'énergie sur ledit substrat et à maintenir de façon stable ledit faisceau focalisé en un point de celui-ci pendant un intervalle de temps établi, ledit faisceau amenant la décomposition dudit composé organique audit point où ledit faisceau est incident sur ledit substrat, d'où il résulte que les couches successives de produit de décomposition dudit composé à base organique peuvent croître à partir dudit substrat dans la direction dudit faisceau, afin de produire une structure de pointe à l'échelle nanométrique à allongement élevé, rigide,
    le dépôt d'une couche métallique sur la surface de ladite structure à allongement élevé, dans lequel ladite couche métallique présente des propriétés magnétiques et a une dimension qui contraint ladite pointe à présenter un domaine magnétique unique.
  11. Procédé selon la revendication 10 dans lequel ledit faisceau d'énergie est un faisceau d'électrons (22).
  12. Procédé selon la revendication 11, dans lequel les détails géométriques de ladite structure de pointe sont commandés par la taille du faisceau et l'énergie de faisceau incident dudit faisceau d'électrons.
  13. Procédé selon l'une quelconque des revendications 10 à 12, dans lequel ledit composé organique volatil est choisi parmi la classe des alliages organométalliques.
EP91117499A 1990-10-31 1991-10-14 Sonde d'échelle nanomètre pour microscope à force atomique, et méthode de fabrication Expired - Lifetime EP0483579B1 (fr)

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US60804390A 1990-10-31 1990-10-31
US608043 1990-10-31

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EP0483579A2 EP0483579A2 (fr) 1992-05-06
EP0483579A3 EP0483579A3 (fr) 1992-12-30
EP0483579B1 true EP0483579B1 (fr) 1995-12-27

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US8790462B2 (en) 2003-04-04 2014-07-29 Qunano Ab Precisely positioned nanowhiskers and nanowhisker arrays and method for preparing them

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EP0483579A3 (fr) 1992-12-30
DE69115847D1 (de) 1996-02-08
JPH04233406A (ja) 1992-08-21
EP0483579A2 (fr) 1992-05-06
DE69115847T2 (de) 1996-07-11
JPH081382B2 (ja) 1996-01-10

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